A variable-temperature high-pressure gas plug-in for a closed-cycle cryostat

Abstract

A variable-temperature high-pressure gas plug-in for a closed-cycle cryostat, comprising: a control mechanism, including: a control valve; a gas transmission mechanism, including: a gas transmission pipe, a gas transmission heating component, a plug-in, and a sealed connection component; the plug-in is provided with a through-channel, the gas transmission pipe is disposed in the through-channel, and the gas transmission pipe is communicated with the control valve; the gas transmission heating component heats the gas transmission pipe; the sealed connection component is arranged on the plug-in, and the plug-in is used for being inserted into a jack of the closed-cycle cryostat; a sample storage mechanism, including: a pressure-bearing body, a plugging component, and a sample heating component; an internal portion of the pressure-bearing body has a sample storage space for storing a sample. High-pressure gas is conveyed to the sample storage space through the gas transmission pipe to pressurize the sample, and the sample storage space is heated through the sample heating component, so as to couple the neutron scattering experimental conditions of high and low temperatures and high pressure, and by virtue of the characteristic that the high-pressure gas does not generate a pressure gradient, the sample can obtain uniform pressure, thereby improving the accuracy of the experimental result.

Description

Technical Field

[0001] The present invention relates to the research field related to the coupling of high and low temperature environments and high-pressure gas environments, and particularly relates to a variable-temperature high-pressure gas plug-in for a closed-cycle cryostat. Background Art

[0002] When using a neutron beam to study substances in a high-pressure and low-temperature environment, it is possible to analyze the substances themselves as well as the reaction and synthesis processes of the substances. Therefore, the two basic physical quantities of temperature and pressure are irreplaceable by other physical quantities in the study of influencing factors in material science. In general research, only the influence of a single factor of temperature or pressure on substances can be carried out, and the coupling of multi-field conditions is challenging.

[0003] In a high-pressure environment, solid media and liquid media are usually used as pressure-transmitting media to increase the pressure on substances. Because solid media and liquid media have a relatively small volume compression ratio and are relatively safe to use, their disadvantage is that their hydrostatic performance is relatively poor. In some applications, gas media are used as pressure-transmitting media in high-pressure environments because gas media have good fluidity, good hydrostatic effects, and will not cause a pressure gradient on the sample. By pressurizing the gas medium, the pressure is transmitted to the sample to achieve the purpose of the sample reaching high pressure. However, the disadvantage of gas media is that high-pressure gases are difficult to seal, especially when using helium gas as the medium; moreover, gas media are prone to liquefaction or solidification under low-temperature conditions. Summary of the Invention

[0004] The main technical problem to be solved by the present invention is to achieve the sealing of high-pressure gases, the control under high and low temperature experimental conditions, and the coupling of the two fields of temperature and pressure to meet the needs of a multi-field coupling sample environment and provide a rich environment for the study of material science.

[0005] The present application provides a variable-temperature high-pressure gas plug-in for a closed-cycle cryostat, including:

[0006] A control mechanism, including: a control valve, the inlet end of the control valve is used to externally connect a vacuum pumping device or a preset high-pressure gas source;

[0007] A gas transmission mechanism, including: a gas transmission pipe, a gas transmission heating component, a plug-in, and a sealing connection component; the plug-in is provided with a through-channel, the gas transmission pipe is inserted into the through-channel, both ends of the gas transmission pipe are exposed outside the through-channel, and the gas transmission pipe is sealed with both channel openings of the through-channel; one end of the gas transmission pipe is communicated with the outlet end of the control valve; the gas transmission heating component is used to heat the gas transmission pipe; the sealing connection component is arranged on the plug-in, the plug-in is used to be inserted into the jack of the closed-cycle cryostat, and the sealing connection component is used to seal and connect the plug-in with the orifice of the jack of the closed-cycle cryostat;

[0008] The sample storage mechanism includes: a pressure-bearing body, a plugging component, and a sample heating component; an internal sample storage space is provided in the pressure-bearing body, and a communication channel and a sample injection channel that are both communicated with the sample storage space are further provided on the pressure-bearing body. The other end of the gas transmission pipe is fixedly and sealingly connected to the communication channel, and the plugging component is detachably connected to the sample injection channel; the sample heating component is used to heat the sample storage space.

[0009] According to the variable-temperature high-pressure gas plug-in for a closed-cycle cryostat in the above embodiment, high-pressure gas is transported to the sample storage space through a gas transmission pipe to pressurize the sample, and the sample storage space is heated by the sample heating component, so as to couple the neutron scattering experimental conditions of high and low temperatures and high pressure, and utilize the characteristic that high-pressure gas does not generate a pressure gradient, so that the sample can obtain uniform pressure, thereby improving the accuracy of experimental results. Description of the Drawings

[0010] Figure 1 It is a schematic structural diagram of the variable-temperature high-pressure gas plug-in for a closed-cycle cryostat provided by the present application Figure 1 ;

[0011] Figure 2 It is a schematic structural diagram of the variable-temperature high-pressure gas plug-in for a closed-cycle cryostat provided by the present application Figure 2 ;

[0012] Figure 3 It is a schematic diagram of the structure of the variable-temperature high-pressure gas plug-in for a closed-cycle cryostat provided by the present application after removing the plug-in;

[0013] Figure 4 It is a sectional view of the sample storage mechanism in the variable-temperature high-pressure gas plug-in for a closed-cycle cryostat provided by the present application;

[0014] Figure 5 It is a schematic diagram of the variable-temperature high-pressure gas plug-in for a closed-cycle cryostat provided by the present application applied to a closed-cycle cryostat;

[0015] Figure 6 is Figure 5 sectional view. Detailed Embodiments

[0016] The present invention will be further described in detail below in conjunction with the accompanying drawings through specific embodiments. Similar elements in different embodiments are denoted by related similar element numbers. In the following embodiments, many detailed descriptions are provided to enable a better understanding of the present application. However, those skilled in the art can easily recognize that some of the features can be omitted in different situations, or can be replaced by other elements, materials, or methods. In some cases, some operations related to the present application are not shown or described in the specification to avoid overwhelming the core part of the present application with excessive descriptions. For those skilled in the art, it is not necessary to describe these related operations in detail, and they can fully understand the related operations based on the descriptions in the specification and general technical knowledge in the art.

[0017] In addition, the features, operations, or characteristics described in the specification can be combined in any suitable manner to form various embodiments. At the same time, the steps or actions in the method description can also be reordered or adjusted in an obvious manner by those skilled in the art. Therefore, the various sequences in the specification and drawings are only for clearly describing a certain embodiment and do not mean that they are necessary sequences, unless it is stated that a certain sequence must be followed.

[0018] The serial numbers assigned to the components in this document, such as "first", "second", etc., are only used to distinguish the described objects and do not have any sequential or technical meanings. The terms "connection" and "coupling" used in this application, unless otherwise specified, both include direct and indirect connections (couplings).

[0019] The present application provides a variable-temperature high-pressure gas plug-in for a closed-cycle cryostat, mainly providing an experimental environment with high pressure and coupling of high and low temperatures for neutron scattering experiments. By using a neutron beam to study samples (such as materials) and the reaction and synthesis processes of samples, high-pressure gas is transported into the sample storage space through a gas pipeline to pressurize the sample, so that the sample is in a high-pressure environment. The sample storage space is heated by a sample heating component to make the sample in a controllable high and low temperature environment. In this way, not only can the needs of a sample environment with coupled high and low temperatures and high pressure be met, but also, by utilizing the characteristic that high-pressure gas does not generate a pressure gradient, the sample can obtain uniform pressure.

[0020] See Figures 1 - 4As shown in the figure, the variable-temperature high-pressure gas plug-in for a closed-cycle cryostat provided in this embodiment includes: a control mechanism 10, a gas transmission mechanism 20, and a sample storage mechanism 30. A sample is stored in the sample storage mechanism 30. Placing the sample storage mechanism 30 inside the closed-cycle cryostat 100 can provide a low-temperature environment for the sample. The control mechanism 10 can connect an external vacuum pumping device or a preset high-pressure gas source to the gas transmission mechanism 20. Through the control of the control mechanism 10, the gas transmission mechanism 20 can evacuate the sample storage space in the sample storage mechanism 30 or input high-pressure gas to pressurize it. The sample storage mechanism 30 can also heat the sample in the sample storage space, so as to meet the variable-temperature high-pressure environment required for neutron scattering experiments.

[0021] The control mechanism 10 includes: a control valve 11. The control valve 11 has an inlet end and an outlet end. The inlet end of the control valve 11 is used to connect an external vacuum pumping device or a preset high-pressure gas source. The control valve 11 adopts a needle valve, and the needle valve has an open state and a closed state. In the open state, the external vacuum pumping device or the preset high-pressure gas source can be connected to the sample storage space through the gas transmission pipe to evacuate the sample storage space by the vacuum pumping device, or pressurize the sample in the sample storage space with the high-pressure gas generated by the preset high-pressure gas source. In the closed state, it is disconnected from the external vacuum pumping device or the preset high-pressure gas source.

[0022] The gas transmission mechanism 20 includes: a gas transmission pipe 21, a gas transmission heating component 22, a plug-in 23, and a sealing connection component 24. A through-channel (not shown in the figure) runs through the inside of the plug-in 23, and the gas transmission pipe 21 is threaded through the through-channel. Both ends of the gas transmission pipe 21 are exposed outside the through-channel, and the gas transmission pipe 21 is sealed with the two channel openings of the through-channel. One end of the gas transmission pipe 21 is connected to the outlet end of the control valve 11. The sample storage space is evacuated by the vacuum pumping device connected to the inlet end of the control valve 11, or high-pressure gas is provided to the sample in the sample storage space through the preset high-pressure gas source connected to the inlet end of the control valve 11 to pressurize the sample. The gas transmission heating component 22 is used to heat the gas transmission pipe 21. The sealing connection component 24 is arranged on the plug-in 23. The plug-in 23 is used to be inserted into the jack 101 of the closed-cycle cryostat 100, and the sealing connection component 24 is used to seal and connect the plug-in 23 to the orifice of the jack 101 of the closed-cycle cryostat 100, so that the sample can be in a low-temperature environment that meets the requirements of neutron scattering experiments through the closed-cycle cryostat 100.

[0023] In this embodiment, the gas pipeline 21 is sealed with the through-channel of the plug-in member 23, preventing external air from entering the through-channel, thereby avoiding the liquefaction or solidification of the high-pressure gas introduced through the externally connected preset high-pressure gas source, and ensuring that the sample can receive a uniform pressurizing effect. At the same time, since the plug-in member 23 is inserted into the closed-cycle cryostat and is in a low-temperature environment, heating the gas pipeline 21 through the gas pipeline heating assembly 22 can also avoid the liquefaction or solidification of the high-pressure gas.

[0024] In a preferred embodiment, the gas pipeline heating assembly 22 generally uses heating wires, which are wound around the outer wall of the gas pipeline 21 in a spiral manner along the length direction of the gas pipeline 21. On the one hand, it ensures that the gas pipeline 21 is evenly heated, avoiding the solidification of the high-pressure gas into liquid or solid in a low-temperature environment, and thereby avoiding the sample from being subjected to a pressure with a gradient change, improving the accuracy of the experiment. On the other hand, it can save the installation space of the heating wires. Of course, in other embodiments, the gas pipeline heating assembly 22 can also adopt other methods and be arranged in the through-channel, and can also heat the gas pipeline 21.

[0025] In one embodiment, the plug-in member 23 is rod-shaped, and a through-channel penetrating the plug-in member 23 is provided at the center of the plug-in member 23 along the length direction of the rod-shaped structure. In a preferred embodiment, the center line of the through-channel coincides with the axis line of the rod-shaped plug-in member 23. In this embodiment, the plug-in member 23 is tubular, and the inner tube of the tubular plug-in member 23 is the through-channel. Both ends of the through-channel are of a port type structure, and the gas pipeline 21 and the plug-in member 23 are coaxial.

[0026] In this embodiment, a vacuum sealing assembly 28 is provided at one channel opening of the through-channel. In the vacuum sealing assembly 28 through which the gas pipeline 21 passes, a sealing effect can be achieved. Of course, in other embodiments, vacuum sealing assemblies can be provided at both channel openings of the through-channel.

[0027] See Figure 3 As shown, the gas delivery mechanism 20 further includes: a gas delivery temperature detection and regulation unit 25. The output end of the gas delivery temperature detection and regulation unit 25 is electrically connected to the input end of the gas pipeline heating assembly 22. The gas delivery temperature detection and regulation unit 25 is used to detect the temperature of the gas pipeline 21 and adjust the heating temperature of the gas pipeline heating assembly 22 according to the preset gas delivery temperature.

[0028] In this embodiment, the gas transmission temperature detection and regulation unit 25 compares the detected temperature of the gas transmission pipe 21 with the preset gas transmission temperature. When the detected temperature of the gas transmission pipe 21 is lower than the preset gas transmission temperature, the power of the gas transmission heating component 22 is increased to increase the heating temperature of the gas transmission heating component 22; when the detected temperature of the gas transmission pipe 21 is higher than the preset gas transmission temperature, the power of the gas transmission heating component 22 is decreased to decrease the heating temperature of the gas transmission heating component 22. Thus, the heating power of the gas transmission heating component 22 is regulated.

[0029] In some embodiments, the preset gas transmission temperature can be a certain temperature range interval.

[0030] Continue to refer to Figure 3 As shown, a fixing block is further provided on the gas transmission pipe 21, and the gas transmission temperature detection and regulation unit 25 is arranged on the fixing block. The fixing block includes a first half fixing member 263 and a second half fixing member 264, and the first half fixing member 263 and the second half fixing member 264 are fixed on the gas transmission pipe 21 in a hoop shape.

[0031] Refer to Figures 1 - 4 As shown, the sample storage mechanism 30 includes: a pressure-bearing body 31, a plugging component 32, and a sample heating component 33. The pressure-bearing body 31 is a structure capable of withstanding high pressure, such as Figure 4 As shown, the pressure-bearing body 31 has a sample storage space 310 inside, and the sample storage space 310 is used to store samples. The sample can be a certain material, and neutron scattering experiments are carried out on the sample through the neutron scattering effect to analyze the reaction and synthesis process of the sample, and further obtain the structural characteristics of the sample. A communication channel 311 and a sample injection channel 312 are also provided on the pressure-bearing body 31. Both the communication channel 311 and the sample injection channel 312 are communicated with the sample storage space 310. The other end of the gas transmission pipe 21 is fixedly and hermetically connected to the communication channel 311. The plugging component 32 is detachably connected to the sample injection channel 312. When the plugging component 32 is installed in the sample injection channel 312, the sample injection channel 312 can be hermetically plugged. After the plugging component 32 is detached from the sample injection channel 312, the sample can be put into the sample storage space 310 through the sample injection channel 312. The sample heating component 33 is used to heat the sample storage space 310, so that the sample can be in a high-temperature environment.

[0032] In one embodiment, the sample heating component 33 can be arranged in the sample storage space 310 to directly heat the sample. Or, the sample heating component 33 is arranged on the pressure-bearing body 31, and the pressure-bearing body 31 is made of a material that can withstand high pressure and conduct heat, so as to heat the sample storage space 310 by heat conduction.

[0033] In this embodiment, the plugging assembly 32 includes a plugging nut 321 and a plugging steel ball 322. The sampling channel 312 is provided with a threaded section, and the plugging nut 321 can be screwed into the threaded section. A conical groove 313 is provided at the connection between the sampling channel 312 and the sample storage space 310. The plugging steel ball 322 is placed in the conical groove 313, and the plugging steel ball 322 is pressed tightly in the conical groove 313 by the plugging nut 321. By utilizing the smoothness of the surface of the plugging steel ball 322 to press tightly against the conical groove 313, the contact area between the plugging steel ball 322 and the conical groove 313 can be increased, achieving a sealing effect.

[0034] Continue to refer to Figure 4 As shown, a screw sleeve 323 is provided on the channel wall of the communication channel 311. A nut 324 is screwed into the screw sleeve 323. A through hole penetrating the axial direction of the nut is provided inside the nut 324, and the through hole is coaxial with the communication channel 311. The other end of the gas transmission pipe 21 is inserted into the through hole. In this embodiment, the end of the other end of the gas transmission pipe 21 can also adopt a conical shape to increase the contact area to ensure airtightness.

[0035] As Figures 1 - 3 shown, in this embodiment, the sample storage mechanism 30 further includes a sample temperature detection and regulation unit 34. The output end of the sample temperature detection and regulation unit 34 is electrically connected to the input end of the sample heating assembly 33. The sample temperature detection and regulation unit 34 is used to detect the temperature of the sample storage space 310 and adjust the heating temperature of the sample heating assembly 33 according to the preset sample temperature.

[0036] In this embodiment, the sample temperature detection and regulation unit 34 compares the detected temperature of the sample storage space 310 with the preset sample temperature. When the detected temperature of the sample storage space 310 is lower than the preset sample temperature, the power of the sample heating assembly 33 is increased to increase the heating temperature of the sample heating assembly 33; when the detected temperature of the sample storage space 310 is higher than the preset sample temperature, the power of the sample heating assembly 33 is decreased to lower the heating temperature of the sample heating assembly 33. Thus, the heating power of the sample heating assembly 33 is regulated.

[0037] In some embodiments, the preset sample temperature can also be a certain temperature range interval.

[0038] In this embodiment, there are two sample temperature detection and regulation units 34 and two sample heating assemblies 33. The two sample temperature regulation units 34 and the two sample heating assemblies 33 are symmetrically arranged respectively. The symmetric arrangement helps the two sample heating assemblies 33 to uniformly heat the sample storage space 310. At the same time, the symmetric arrangement helps the two sample temperature detection and regulation units 34 to obtain accurate detection temperatures, making the experimental data more accurate.

[0039] In one embodiment, two hoops 35 are further arranged outside the pressure-bearing body 31, and two sample temperature control units 34 and two sample heating assemblies 33 are symmetrically arranged on the two hoops 35 respectively.

[0040] Continue to refer to Figures 1 - 3 As shown, the variable-temperature high-pressure gas plug-in for a closed-cycle cryostat provided in this application further includes: a temperature-measuring connection plug 40 and a heating connection plug 50. The temperature-measuring connection plug 40 is electrically connected to the gas-transporting temperature detection and control unit 25 and the two sample temperature detection and control units 34, so as to connect the gas-transporting temperature detection and control unit 25 and the two sample temperature detection and control units 34 to an external display device through the temperature-measuring connection plug 40, and display the temperature values measured by the gas-transporting temperature detection and control unit 25 and the two sample temperature detection and control units 34 through the display device. The heating connection plug 50 is electrically connected to the gas-transporting heating assembly 22 and the sample heating assembly 33, so as to connect the gas-transporting heating assembly 22 and the sample heating assembly 33 to an external power supply through the heating connection plug 50, and supply power to the gas-transporting heating assembly 22 and the sample heating assembly 33 through the external power supply to ensure their normal operation.

[0041] In this embodiment, the sealing connection assembly 24 is of a flange structure. The temperature-measuring connection plug 40 and the heating connection plug 50 are both arranged on the upper surface 241 of the flange-structured sealing connection assembly 24. This upper surface is exposed outside the closed-cycle cryostat after inserting this plug-in into the closed-cycle cryostat, so as to facilitate connection with an external display device and power supply.

[0042] In some embodiments, the variable-temperature high-pressure gas plug-in for a closed-cycle cryostat provided in this application may further include: a controller. The gas-transporting temperature detection and control unit 25 and the sample temperature detection and control unit 34 are both electrically connected to the input end of the controller, and the gas-transporting heating assembly 22 and the sample heating assembly 33 are both electrically connected to the output end of the controller. The temperature of the gas-transporting pipe 21 detected by the gas-transporting temperature detection and control unit 25 can be output to the controller. The controller can generate a corresponding control signal according to the detected temperature of the gas-transporting pipe 21 and the preset gas-transporting temperature, and output this control signal to the gas-transporting heating assembly 22 to adjust the heating power of the gas-transporting heating assembly 22. Similarly, the temperature of the sample storage space 310 detected by the sample temperature detection and control unit 34 can be output to the controller. The controller can generate a corresponding control signal according to the detected temperature of the sample storage space 310 and the preset sample temperature, and output the control signal to the sample heating assembly 33 to adjust the heating power of the sample heating assembly 33.

[0043] The variable-temperature high-pressure gas plug-in for a closed-cycle cryostat provided by this application further includes: a displacement adjustment mechanism 60. In this embodiment, the gas delivery pipe 21 can reciprocally slide relative to the two channel openings of the through-channel. For example, the sealing components provided at the two channel openings of the through-channel are both sealing rings. Through the sealing rings, not only can the sealing effect be achieved, but at the same time, the gas delivery pipe 21 can also reciprocally slide relative to the sealing rings. Both the control valve 11 and the plug-in 23 are connected to the displacement adjustment mechanism 60, and the displacement adjustment mechanism 60 is used to drive the gas delivery pipe 21 to reciprocally move relative to the through-channel, so as to change the position of the pressure-bearing body 31.

[0044] In some embodiments, the sealing connection assembly 24 is arranged at one end of the plug-in 23 close to the control valve 11, and the sealing connection assembly 24 is connected to the displacement adjustment mechanism 60, so that the plug-in 23 is indirectly connected to the displacement adjustment mechanism 60.

[0045] In this embodiment, the gas delivery pipe 21 and the through-channel maintain a coaxial relationship. The displacement adjustment mechanism 60 drives the gas delivery pipe 21 to reciprocally move along the axis of the through-channel. Since the control valve 11 is fixedly connected to one end of the gas delivery pipe 21 and the pressure-bearing body 31 is hermetically fixed to the other end of the gas delivery pipe 21, the gas delivery pipe 21 reciprocally moving along the axis of the through-channel can drive the pressure-bearing body 31 to reciprocally move synchronously, so as to change the relative position of the pressure-bearing body 31, that is, change the relative position of the sample storage space 310. When performing a neutron scattering experiment, if the number of samples stored in the sample storage space 310 is small and the samples can only be at the bottom of the sample storage space 310, by changing the position of the pressure-bearing body 31, the position of the samples in the sample storage space 310 can be changed, and the samples can be moved to the center of the neutron beam to ensure that the central flux of the neutron beam passing through the samples is the highest, improving the experimental efficiency and the accuracy of the experimental results.

[0046] In this embodiment, the displacement adjustment mechanism 60 includes: a fixed part 61 and a sliding part 62. The control valve 11 is arranged on the sliding part 62, the plug-in 23 is connected to the fixed part 61, and the sliding part 62 can reciprocally slide relative to the fixed part 61, so as to drive the gas delivery pipe 21 to reciprocally slide relative to the through-channel, and further change the relative position of the pressure-bearing body 31.

[0047] In some embodiments, a slide rail is arranged on the fixed part 61, a slider is arranged on the sliding part 62, the slider is slidably arranged on the slide rail, and the slide rail can guide the direction of the reciprocal sliding.

[0048] Such as Figures 1 - 3As shown, the control mechanism 10 further includes: a safety valve 12, which is connected between the outlet end of the control valve 11 and one end of the gas transmission pipe 21. Specifically, the safety valve 12 is connected to the outlet end of the control valve 11 through a communication pipeline 110, and the inlet end of the control valve 11 is connected to one end of the gas transmission pipe 21 through a connection pipeline 120. A rupture disc capable of withstanding a preset pressure range is provided inside the safety valve 12. The safety valve 12 is used to relieve pressure when the air pressure in the gas transmission pipe 21 is greater than the preset pressure range, so as to avoid the risk of explosion of the gas transmission pipe 21 when the internal air pressure is greater than the preset pressure, and improve the safety of the equipment.

[0049] In the above embodiment, since the control valve 11 needs to be frequently operated, the diameter of the connection pipeline 120 adopted should be larger than that of the gas transmission pipe 21. The connection pipeline 120 with a larger diameter is firm and durable, and can reduce the risk of gas leakage. Therefore, to ensure the connection between the connection pipeline 120 and the gas transmission pipe 21, the control mechanism 10 further includes: a reducer joint 13, which is arranged between the safety valve 12 and one end of the gas transmission pipe 21.

[0050] In this embodiment, both the safety valve 12 and the reducer joint 13 are arranged on the sliding member 62, which can not only ensure the effective connection with the control valve 11, but also save the connection pipeline cost between components. Of course, on the premise of not considering the connection effect and cost, the safety valve 12 and the reducer joint 13 can also be connected to other structures. Correspondingly, to ensure that the control valve 11 can move synchronously with the sliding member 62, the corresponding communication pipeline 110 and connection pipeline 120 can adopt a sufficient length, or adopt a sufficient degree of flexible hose.

[0051] In some embodiments, to facilitate the measurement of the vacuum degree and high-pressure gas, a vacuum degree detection component and a gas pressure detection component can also be provided on the communication pipeline 110 and / or the connection pipeline 120. The vacuum degree detection component usually adopts a vacuum gauge, which can measure the vacuum degree of the sample storage space 310 after the external vacuum pumping equipment pumps the vacuum, and complete the vacuum pumping operation when the preset vacuum degree is reached. The gas pressure detection component usually adopts a pressure gauge, which can supply high-pressure gas to the sample storage space 310 from an external preset high-pressure gas source and complete the delivery of high-pressure gas when the preset pressure is reached.

[0052] In this embodiment, the gas delivery mechanism 20 further includes: a plurality of heat insulation members 27, each heat insulation member 27 is arranged on the plug-in member 23 at equal intervals, and all the heat insulation members 27 are located between the sealed connection assembly 24 and the other end of the gas delivery pipe 21. After the plug-in member 23 is inserted into the jack 101 of the closed-cycle cryostat 100, each heat insulation member 27 supports on the inner wall of the jack 101 of the closed-cycle cryostat 100, and all the heat insulation members 27 are used to block the heat conduction between the jack 101 and the plug-in member 23, avoiding the heat conduction between the closed-cycle cryostat 100 and the plug-in member 23. This can not only ensure that the preset air pressure gas source in the gas delivery pipe 21 does not solidify into a liquid or solid, but also effectively save the heating amount of the gas delivery heating assembly 22 and reduce costs.

[0053] In one embodiment, the gas delivery mechanism 20 further includes: a positioning and buffering assembly 26, and the positioning and buffering assembly 26 is used to position and buffer the plug-in member 23 when the plug-in member 23 is inserted into the jack 101 of the closed-cycle cryostat 100.

[0054] In this embodiment, the positioning and buffering assembly 26 includes: a sliding heat conducting member 261 and an elastic buffering member 262. A limiting portion 231 is further arranged on the plug-in member 23, the sliding heat conducting member 261 is slidably arranged on the plug-in member 23, and the sliding heat conducting member 261 is located between the limiting portion 231 and the heat insulation member 27 closest to the pressure-bearing body 31. Taking the plug-in member 23 as the vertical direction as an example, the heat insulation member 27 closest to the pressure-bearing body 31 is the bottommost heat insulation member 27. The sliding heat conducting member 261 is used to be clamped in the jack 101 of the closed-cycle cryostat 100 and conduct heat with the pressure-bearing body 31. The elastic buffering member 262 is arranged between the sliding heat conducting member 261 and the heat insulation member 27 close to the pressure-bearing body 31, and is used to buffer the sliding heat conducting member 261.

[0055] In the above embodiment, the sliding heat conducting member 261 is a sliding heat conducting member with a cylindrical structure, the elastic buffering member 262 is a spring, and both the sliding heat conducting member with a cylindrical structure and the spring are sleeved on the plug-in member 23.

[0056] The working process of the variable-temperature high-pressure gas plug-in for the closed-cycle cryostat provided by this application is as follows:

[0057] Open the plugging nut 321, remove the plugging steel ball 322, load the sample into the interior of the sample storage space 310 through the sample injection channel 312, put in the plugging steel ball 322, and re-screw the plugging nut 321 onto the sample injection channel 312.

[0058] Insert the plug-in 23 into the jack 101 of the closed-loop cryostat 100, and sealingly connect the sealing connection assembly 24 to the orifice of the jack 101. Then turn on the closed-loop cryostat 100. Connect an external vacuum pumping device through the control valve 11. Start the vacuum pumping device and open the control valve 11 to evacuate the sample storage space 310. After reaching the required vacuum degree, close the control valve 11 and remove the vacuum pumping device.

[0059] Turn on the heating function of the gas transmission heating assembly 22 to heat the gas transmission pipe 21. The gas transmission temperature detection and regulation unit 25 detects the heating temperature of the gas transmission heating assembly 22 and regulates the heating power of the gas transmission heating assembly 22 according to the preset gas transmission temperature to prevent the high-pressure gas from solidifying into liquid or solid.

[0060] Turn on the heating function of the sample heating assembly 33 to heat the sample storage space 310. The sample temperature detection and regulation unit 34 detects the heating temperature of the sample heating assembly 33 and regulates the heating power of the sample heating assembly 33 according to the preset sample temperature to make it reach the temperature required for neutron scattering experiments.

[0061] Connect an external preset high-pressure gas source to the control valve 11. Open the control valve to inject high-pressure gas (the type of gas can be selected according to the experimental requirements) into the sample storage space 310. When the pressure required for neutron scattering experiments is reached, close the control valve 11.

[0062] Turn on the beam device to provide a neutron beam to the sample in the sample storage space 310 for neutron scattering experiments.

[0063] After the experiment is completed, open the control valve 11 to discharge the high-pressure gas, and turn off the gas transmission heating assembly 22 and the sample heating assembly 33. Pull out the plug-in 23, remove the plugging nut 321 and the plugging steel ball 322, and take out the stored sample to complete the experiment.

[0064] It should be noted that during the experiment, the gas transmission temperature detection and regulation unit 25 and the sample temperature detection and regulation unit 34 respectively detect and regulate the temperatures of the gas transmission heating assembly 22 and the sample heating assembly 33 in real time.

[0065] In summary, the variable-temperature high-pressure gas plug-in for the closed-loop cryostat provided in this embodiment transports high-pressure gas to the sample storage space through the gas transmission pipe to pressurize the sample, and heats the sample storage space through the sample heating assembly, thereby coupling the neutron scattering experimental conditions of high and low temperatures and high pressure, and utilizing the characteristic that high-pressure gas does not generate a pressure gradient, so that the sample can obtain uniform pressure, and further improving the accuracy of the experimental results.

[0066] The above uses specific examples to illustrate the present invention, which is only for helping to understand the present invention and is not intended to limit the present invention. For those skilled in the art of the present invention, based on the idea of the present invention, several simple deductions, deformations or substitutions can also be made.

Claims

1. A variable-temperature high-pressure gas plug-in for a closed-cycle cryostat, characterized in that Comprising: A control mechanism, comprising: a control valve, the inlet end of the control valve is used to externally connect a vacuum pumping device or a preset high-pressure gas source; A gas transmission mechanism, comprising: a gas transmission pipe, a gas transmission heating component, a plug, and a sealing connection component; the plug is provided with a through-channel, the gas transmission pipe is disposed through the through-channel, both ends of the gas transmission pipe are exposed outside the through-channel, and seals are provided between the two channel openings of the through-channel and the gas transmission pipe; one end of the gas transmission pipe is communicated with the outlet end of the control valve; the gas transmission heating component is used to heat the gas transmission pipe; the sealing connection component is disposed on the plug, the plug is used to be inserted into the jack of the closed-cycle low-temperature thermostat, and the sealing connection component is used to seal and connect the plug with the orifice of the jack of the closed-cycle low-temperature thermostat; A sample storage mechanism, comprising: a pressure-bearing body, a plugging component, and a sample heating component; the interior of the pressure-bearing body has a sample storage space for storing samples, the pressure-bearing body is further provided with a communication channel and a sample injection channel both communicated with the sample storage space, the other end of the gas transmission pipe is fixedly and hermetically connected with the communication channel, and the plugging component is detachably connected to the sample injection channel; the sample heating component is used to heat the sample storage space; Further comprising: a displacement adjustment mechanism, the gas transmission pipe can reciprocally slide relative to the two channel openings of the through-channel, both the control valve and the plug are connected to the displacement adjustment mechanism, and the displacement adjustment mechanism is used to drive the gas transmission pipe to reciprocally move relative to the through-channel so as to change the position of the pressure-bearing body.

2. The variable-temperature high-pressure gas plug-in for a closed-cycle cryostat according to claim 1, wherein, The displacement adjustment mechanism comprises: a fixed member and a sliding member, the control valve is disposed on the sliding member, the plug is connected to the fixed member, and the sliding member can reciprocally slide relative to the fixed member.

3. The variable-temperature high-pressure gas plug-in for a closed-cycle cryostat according to claim 1, wherein The gas transmission mechanism further comprises: a gas transmission temperature detection and regulation unit, the output end of the gas transmission temperature detection and regulation unit is electrically connected to the input end of the gas transmission heating component, and the gas transmission temperature detection and regulation unit is used to detect the temperature of the gas transmission pipe and regulate the heating temperature of the gas transmission heating component according to a preset gas transmission temperature.

4. The variable-temperature high-pressure gas plug-in unit for a closed-cycle cryostat according to claim 1, wherein, The sample storage mechanism further comprises: a sample temperature detection and regulation unit, the output end of the sample temperature detection and regulation unit is electrically connected to the input end of the sample heating component, and the sample temperature detection and regulation unit is used to detect the temperature of the sample storage space and regulate the heating temperature of the sample heating component according to a preset sample temperature.

5. The variable-temperature high-pressure gas plug-in for a closed-cycle cryostat according to claim 1, characterized in that, The control mechanism further comprises: a safety valve, the safety valve is connected between the outlet end of the control valve and one end of the gas transmission pipe, and is used to relieve pressure when the air pressure in the gas transmission pipe is greater than a preset pressure range.

6. The variable-temperature high-pressure gas plug for a closed-cycle cryostat according to claim 5, characterized in that, The control mechanism further comprises: a reducing joint, the reducing joint is disposed between the safety valve and one end of the gas transmission pipe, a connecting pipeline is further disposed between the safety valve and the reducing joint, and the diameter of the connecting pipeline is larger than the diameter of the gas transmission pipe.

7. The variable-temperature high-pressure gas plug-in for a closed-cycle cryostat according to claim 1, characterized in that, The gas transmission mechanism further includes: a plurality of heat insulation members, which are arranged on the plug at equal intervals and are located between the sealed connection assembly and the other end of the gas transmission pipe; the plurality of heat insulation members are supported on the inner wall of the jack of the closed-cycle cryostat for blocking heat conduction between the jack and the plug.

8. The variable-temperature high-pressure gas plug-in for a closed-cycle cryostat according to claim 7, characterized in that, The gas transmission mechanism further includes: a positioning and buffering assembly, which is used for positioning and buffering the plug when the plug is inserted into the jack of the closed-cycle cryostat.

9. The variable-temperature high-pressure gas plug for a closed-cycle cryostat according to claim 8, characterized in that, The positioning and buffering assembly includes: a sliding heat conducting member and an elastic buffering member; a limiting portion is further arranged on the plug, the sliding heat conducting member is slidably arranged on the plug, and the sliding heat conducting member is located between the limiting portion and the heat insulation member closest to the pressure-bearing body; the sliding heat conducting member is used for being clamped in the jack of the closed-cycle cryostat and conducting heat with the pressure-bearing body; the elastic buffering member is arranged between the sliding heat conducting member and the heat insulation member close to the pressure-bearing body for buffering the sliding heat conducting member.

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